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Combination of Thin-Layer Chromatography and Mass Spectrometry Using Cluster-Induced Desorption/Ionization.

ABSTRACT: Desorption/ionization induced by neutral clusters (DINeC) was employed for mass spectrometry (MS) of oligopeptides and lipids after separation by means of thin-layer chromatography (TLC). Clear and fragmentation-free spectra were obtained from the TLC plates without any further sample treatment. Mass-resolved chromatograms were deduced when scanning the TLC plates with the cluster beam along the direction of solvent movement. Using vancomycin and noncovalently bound complexes, the soft nature of DINeC was demonstrated also when used in combination with TLC. As a test application, TLC and DINeC-MS were employed to separate and detect different phospholipids obtained from egg yolk.

SUBMITTER: Heep J

PROVIDER: S-EPMC6941192 | biostudies-literature | 2019 Dec

REPOSITORIES: biostudies-literature

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Combination of Thin-Layer Chromatography and Mass Spectrometry Using Cluster-Induced Desorption/Ionization.

Heep Julian J Tuchecker Paul H K PHK Gebhardt Christoph R CR Dürr Michael M

ACS omega 20191220 27

Desorption/ionization induced by neutral clusters (DINeC) was employed for mass spectrometry (MS) of oligopeptides and lipids after separation by means of thin-layer chromatography (TLC). Clear and fragmentation-free spectra were obtained from the TLC plates without any further sample treatment. Mass-resolved chromatograms were deduced when scanning the TLC plates with the cluster beam along the direction of solvent movement. Using vancomycin and noncovalently bound complexes, the soft nature of ...[more]

PMID: 31909324

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Project description:We recently reported the use of desorption electrospray ionization (DESI) as a novel interface to couple high-performance liquid chromatography (HPLC) with mass spectrometry (MS) (Chem. Commun. 2011, 47, 4171). One of the benefits of such an interface is that post-column derivatization of separated analytes can be integrated with ionization via a "reactive" DESI approach in which a derivatizing reagent is doped into the spray solvent. The reactive DESI interface allows analyte desorption/ionization from the end of the chromatographic column with prompt MS detection; a short time delay of ~20 ms was demonstrated. In this study, we extended this application by "supercharging" proteins following HPLC separation using a DESI spray solvent containing supercharging reagents, m-nitrobenzyl alcohol (m-NBA) or sulfolane. Proteins (insulin, ubiquitin, lysozyme and α-lactalbumin) eluted out of the LC column can be supercharged with the protein charge state distributions (CSDs) significantly increased (to higher charge), which would be advantageous for subsequent top-down MS analysis of proteins. Interestingly, supercharging combined with reactive DESI enhances tolerance towards trifluoroacetic acid (TFA), which is known to be a superior additive in the mobile phase for premium peptide/protein chromatographic separation but has severe signal suppression effects for conventional electrospray ionization (ESI). In comparison to electrosonic spray ionization (ESSI), a variant form of ESI, the sensitivity of protein analysis using LC/DESI-MS with the mobile phase containing TFA can be improved by up to 70-fold for lysozyme and α-lactalbumin by including m-NBA in the DESI spray solvent. Presumably, by reducing TFA dissociation in the droplet, supercharging agents lower trifluoroacetate anion concentrations and concomitantly reduce ion pairing to analyte cationic sites. The reduced ion pairing therefore decreases the TFA signal suppression effect. The supercharging capability and the reduction of TFA signal suppression suggest that LC/DESI-MS is a valuable method for protein analysis.

Dataset Information

Combination of Thin-Layer Chromatography and Mass Spectrometry Using Cluster-Induced Desorption/Ionization.

Publications

Combination of Thin-Layer Chromatography and Mass Spectrometry Using Cluster-Induced Desorption/Ionization.

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